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以二烯丙基胺、氯乙酸丁酯和K2CO3为原料,合成了N,N-二烯丙基-N-羰丁氧甲基胺(DACBMA),将油相与水相分离后用无水硫酸镁干燥,再减压蒸馏,收集157~161℃/1 333 Pa的馏分;然后将收集的馏分用6 mol/L的盐酸中和至油相消失,得到N,N-二烯丙基-N-羰丁氧甲基氯化铵(DACBMAC)溶液;或将其溶于无水乙醚,通入干燥氯化氢,可得到固体DACBMAC。结果表明,当n(二烯丙基胺)∶n(氯乙酸丁酯)∶n(K2CO3)=1.5∶1∶1,反应温度70℃,氯乙酸丁酯滴加时间60 m in,反应时间8 h时,DACBMA的收率为74.30%;将分离得到的水相和减压蒸馏得到的低沸点馏分回用,其收率可提高到83.23%;与干燥氯化氢季铵化相比,采用盐酸中和反应快,无尾气污染,但不能得到固体产物;DACBMAC收率达81.56%,比干燥氯化氢季铵化高10.51%。用元素分析、FTIR和1HNMR对中间产物和终产物的结构进行了表征。并已进行了1 L规模的扩试。
Diallyl amine, butyl chloroacetate and K2CO3 were used as raw materials to synthesize N, N-diallyl-N-carbobutylmethylamine (DACBMA). The oil phase was separated from the aqueous phase and then treated with anhydrous Dried over magnesium sulfate and then distilled under reduced pressure to collect a fraction of 157-161 ° C / 1 333 Pa. The collected fraction was then neutralized with 6 mol / L hydrochloric acid until the oil phase disappeared to give N, N-diallyl- N-carboethoxymethyl ammonium chloride (DACBMAC) solution; or dissolved in anhydrous ether, access to dry hydrogen chloride to obtain a solid DACBMAC. The results showed that when the reaction time was 60 min, the reaction time was 60 min and the reaction time was 70 ℃. The reaction time The yield of DACBMA was 74.30% at 8 h. The separated aqueous phase and the low-boiling distillate obtained by vacuum distillation were reused to increase the yield to 83.23%. Compared with the quaternization of dry hydrogen chloride, Neutralization reaction, no exhaust pollution, but can not get solid product; DACBMAC yield of 81.56%, 10.51% higher than the dry quaternization of hydrogen chloride. The structures of intermediates and final products were characterized by elemental analysis, FTIR and 1HNMR. And has been a 1 L scale expansion test.